A method for refining thionyl chloride

A technology of thionyl chloride and sulfur dichloride, applied in the directions of thionyl chloride, sulfur and halogen compounds, etc., can solve the problems of low yield and purity of thionyl chloride, instability, low utilization rate of raw materials, etc. The effect of reducing equipment investment, reducing pressure and improving purity

Active Publication Date: 2020-10-09
JIANGXI SELON INDAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, due to the instability of the rectification and purification process in this prior art, and the sulfur complexing reaction does not add any catalyst, the yield and purity of the obtained sulfur oxychloride are low, and the utilization rate of raw materials is low

Method used

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  • A method for refining thionyl chloride
  • A method for refining thionyl chloride
  • A method for refining thionyl chloride

Examples

Experimental program
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Effect test

Embodiment 1

[0049] In this embodiment, the first step of sulfidation reaction is carried out before the mixed gas produced in the thionyl chloride synthesis reactor is condensed. At the same time, a secondary sulfidation bed is set in the rectification device to further purify the crude thionyl chloride to achieve Refining of sulfone.

[0050] The specific method is as follows:

[0051] (1) Synthesis of sulfur dichloride

[0052] Use liquid sulfur monochloride and chlorine to react in the sulfur dichloride synthesis kettle, wherein part of the liquid sulfur monochloride comes from the product generated in the sulfur monochloride reaction kettle, and the other part comes from the high-boiling liquid phase extracted from the rectification tower The volume ratio of chlorine gas to liquid sulfur monochloride is 150:(0.15-0.25), the reaction temperature is controlled at 60-85°C, and the generated SCl 2 and excess Cl 2 The mixed gas is discharged from the gas outlet, and the pressure in the ...

Embodiment 2

[0066] This embodiment adopts the process of Example 1, the difference is that when sulfur is added to the first sulfur compounding kettle, the sulfur is mixed with a desiccant to carry out the first sulfur compounding reaction, and other processes are the same as in Example 1, and the specific methods are as follows:

[0067] (3) The first sulfur matching reaction

[0068] The crude mixed gas produced by the thionyl chloride synthesis kettle is directly passed into the first sulfur compounding kettle without any heating process, and the first sulfur compounding reaction is carried out. The reaction temperature in the first sulfur compounding kettle is from oxychloride to Add sulfur to the residual temperature of the crude product mixed gas discharged from the sulfone synthesis kettle. The method of adding sulfur is: crush the selected sulfur block together with the desiccant calcium chloride particles, and the crushed particles reach 30-50 meshes, and then Send the pulverized...

Embodiment 3

[0071] The present embodiment adopts the technique of embodiment 2, and the difference is that in the first sulfur matching kettle, a catalyst is added to catalyze the first sulfur matching reaction, and other techniques are the same as in example 2, and the specific methods are as follows:

[0072](3) The crude product mixed gas produced by the thionyl chloride synthesis kettle does not directly pass into the first sulfur matching still through any heating process, and carries out the first sulfur matching reaction, and the reaction temperature in the first sulfur matching still is from The residual temperature of the crude product mixed gas discharged from the thionyl chloride synthesis kettle, wherein, an activated carbon bed is arranged in the first sulfur mixing kettle, and the activated carbon is used as a catalyst for the primary vulcanization reaction, and dry sulfur is added thereto, wherein the addition of the sulfur The amount is 70-80% of the amount of sulfur needed...

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Abstract

The invention provides method and equipment for refining of thionyl chloride. A gas mixture generated from a thionyl chloride synthesis kettle is subjected to two steps of sulfur mixing reaction in the process of purifying; particularly, the two steps of sulfur mixing reaction includes firstly, directly introducing the gas mixture discharged from the thionyl chloride synthesis kettle into a firstsulfur mixing kettle for realizing sulfuration, and purifying sulfuretted gas mixture through condensing and degassing to obtain crude thionyl chloride product; secondly, arranging a secondary sulfuration bed on the top of a rectifying apparatus, rectifying and purifying the crude thionyl chloride product for secondary sulfuration, and arranging catalysts in the secondary sulfuration bed. Since the gas discharged from the thionyl chloride synthesis kettle is of high temperature, heating before sulfur mixing reaction is omitted, equipment input is reduced, and decomposition of thionyl chlorideduring heating is reduced; besides, sulfur and drying agents are mixed and added, the circumstance of introducing moisture along with adding of sulfur is avoided, content of impurity of products is reduced, non-condensable gas in the production process is extracted fully, and utilization rate of raw materials is increased.

Description

technical field [0001] The invention relates to the field of chemical technology, in particular to a method for refining thionyl chloride. Background technique [0002] Thionyl chloride is soluble in benzene, chloroform and carbon tetrachloride, decomposes in water to generate sulfurous acid and hydrogen chloride, and decomposes to generate chlorine gas, sulfur dioxide and sulfur monochloride when heated to 140 degrees, and the chlorine atom of thionyl chloride replaces hydroxyl and mercapto It has a strong ability and can sometimes replace sulfur dioxide, oxygen or hydrogen. It can react with organic compounds such as phenols or alcohols with hydroxyl groups to generate corresponding chlorides, react with sulfonic acids to generate sulfonyl chlorides, and react with Grignard reagents to generate corresponding sub- Sulfone compounds, etc. Thionyl chloride is very important in organic synthesis. It is an intermediate raw material for the synthesis of pesticides, medicines, p...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B17/45
CPCC01B17/4584
Inventor 王寿发潘英曙胡美忠
Owner JIANGXI SELON INDAL
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